CN101521276A - Method for producing lithium ion battery positive material coated with carbon - Google Patents
Method for producing lithium ion battery positive material coated with carbon Download PDFInfo
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- CN101521276A CN101521276A CN200910106325A CN200910106325A CN101521276A CN 101521276 A CN101521276 A CN 101521276A CN 200910106325 A CN200910106325 A CN 200910106325A CN 200910106325 A CN200910106325 A CN 200910106325A CN 101521276 A CN101521276 A CN 101521276A
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- lithium ion
- ion battery
- battery positive
- carbon
- positive material
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention relates to a method for producing a lithium ion battery positive material coated with carbon. The method comprises the following steps: a certain amount of lithium ion battery positive material powder is put into polyacrylonitrile solution, the solution is sufficiently stirred and uniformly mixed, after being heated and evaporated, the solution is placed into an oven at an air atmosphere to be heated for 2-4 hours under 150-3000 DEG C so as to obtain black solids, the black solids are placed into a high temperature furnace to be heated for 0.5-4 hours at the temperature of 400-1200 DEG C under the protection of inert gas so as to obtain powdery lithium ion battery positive material coated with carbon on the surface. The lithium ion battery positive material coated with carbon has the advantages of fine particle, uniform carbon coating, good electric conductivity, high specific capacity and good recycling property and has great using value in the field of power type lithium ion batteries.
Description
Technical field
The present invention relates to a kind of preparation method of lithium ion battery positive material coated with carbon, belong to energy and material and technical field of new material preparation.
Background technology
Lithium ion battery is the green high-capacity battery of a new generation, have in light weight, advantages such as volumetric specific energy is high, operating voltage is high, non-environmental-pollution, it is the desirable chemical power source of modern communication, IT and portable type electronic product (as mobile phone, notebook computer, video camera etc.), also be the preferred electrical source of power of following electric automobile, have broad application prospects and huge economic benefit.
Positive electrode is a critical material of making lithium rechargeable battery, is the principal element of decision lithium ion battery performance and price.Therefore, the research and development of anode material for lithium-ion batteries always are forward position and hot subject, are subjected to the great attention of the many advanced countries in the world.
The research and development of anode material for lithium-ion batteries at present mainly concentrate on lithium-compound transition metal oxide positive electrode aspect, mainly comprise LiCoO
2, LiFePO
4, LiNiO
2, LiV
3O
8And LiMn
2O
4And their derivative.These positive electrodes respectively have the advantage of oneself, as: LiCoO
2The voltage height, the specific energy height, cyclicity is good, successfully is used on the small-scale lithium ion cell; LiFePO
4Have high theoretical capacity (170mAh/g), good cycle performance, good thermal stability, aboundresources, cheap, environmental friendliness; LiNiO
2Discharge rate low, do not have environmental pollution, electrolyte is required low; LiV
3O
8Have higher specific capacity, and nontoxic, inexpensive; LiMn
2O
4Good stability, pollution-free, the operating voltage height, with low cost, easily synthetic.But these materials all have a common shortcoming, and the intrinsic electronic conductivity that is exactly cell positive material itself is very low, and this has had a strong impact on the large-current electric chemical property and the practical application of this material.Current, researcher is being obtained some progress aspect the research that improves anode material for lithium-ion batteries.Usually the measure of taking has: (1) mixes conductive carbon material or conductive metal particle in the inside of material, and perhaps at particle surface coated with conductive material with carbon element, the source of these material with carbon elements mainly contains: carbon sol, acetylene black, glucose, sucrose and citric acid etc.; (2) doping of metal ion, as mix Mg
2+, Ti
4+, Cr
3+, Al
3+, Cu
2+, Ag
+, Zr
4+, Nb
5+, W
6+Wait and replace partial L i
+, the electronic conductivity of raising material.These top measures all can improve the conductivity of anode material for lithium-ion batteries to a certain extent.
Summary of the invention
The objective of the invention is to propose a kind of preparation method of lithium ion battery positive material coated with carbon, this method can not only make anode material for lithium-ion batteries coat and go up carbon, particle is tiny, it is even to cover carbon, has bigger specific area, and can improve conductance, specific capacity and the cycle performance of material, realize the practical application of anode material for lithium-ion batteries in the motive-power battery field.
Technical solution of the present invention is as follows:
The certain amount of lithium ion battery positive powder is put into polyacrylonitrile solution; abundant stirring and evenly mixing; behind the heating evaporation solvent; under air atmosphere; put into baking oven and heated 2～4 hours down, obtain black solid, again the black solid of gained is put into high temperature furnace at 150～300 ℃; 400～1200 ℃ were heated 0.5～4 hour under inert gas shielding, just obtained the lithium ion battery powdery positive electrode that the surface has coated carbon.
Above-mentioned anode material for lithium-ion batteries is LiCoO
2, LiFePO
4, LiNiO
2, LiV
3O
8, LiMn
2O
4Or their doped derivatives.
Anode material for lithium-ion batteries LiCoO
2, LiFePO
4, LiNiO
2, LiV
3O
8, LiMn
2O
4Doped derivatives, be partly to replace the compound that is generated behind Co, Fe in the above composite oxides, Ni, V, the Mn with one or more metallic elements among Mg, Ti, Cr, Al, Cu, Ag, Zr, Nb, the W.
The molecular weight of above-mentioned polyacrylonitrile is 1000～30000, and the weight percent concentration of polyacrylonitrile solution is 5～100%.
The weight ratio of above-mentioned polyacrylonitrile and lithium ion battery positive material powder is 25～95%.
Above-mentioned inert gas is nitrogen or argon gas.
The method for preparing lithium ion battery positive material coated with carbon that the present invention set up has the following advantages: the new carbon source that the invention provides a kind of lithium ion battery positive material coated with carbon, it is distributed to the powder of anode material for lithium-ion batteries in the polyacrylonitrile solution, through low temperature pre-oxidation and the high temperature cabonization process under inert gas shielding, carbon on the anode material for lithium-ion batteries surface coats equably; This method technological process is simple; The coating of preparing the powder particle of anode material for lithium-ion batteries of carbon tiny, have bigger specific area; Product has conductivity preferably, large-current electric chemical property excellence; Has very big using value in the power-type lithium ion battery field.
Embodiment
The invention provides a kind of preparation method of lithium ion battery positive material coated with carbon, its concrete processing step is as follows:
The certain amount of lithium ion battery positive powder is put into polyacrylonitrile solution; abundant stirring and evenly mixing; behind the heating evaporation solvent; under air atmosphere; put into baking oven and heated 2～4 hours down, obtain black solid, again the black solid of gained is put into high temperature furnace at 150～300 ℃; 400～1200 ℃ were heated 0.5～4 hour under inert gas shielding, just obtained the lithium ion battery powdery positive electrode that the surface has coated carbon.
Above-mentioned anode material for lithium-ion batteries is LiCoO
2, LiFePO
4, LiNiO
2, LiV
3O
8, LiMn
2O
4Or partly replace the compound that is generated behind Co, Fe in the above composite oxides, Ni, V, the Mn with one or more metallic elements among Mg, Ti, Cr, Al, Cu, Ag, Zr, Nb, the W; The molecular weight of polyacrylonitrile is 1000～30000, and the weight percent concentration of polyacrylonitrile solution is 5～100%; The weight ratio of polyacrylonitrile and lithium ion battery positive material powder is 25～95%; Inert gas is nitrogen or argon gas.
Below by embodiment, further illustrate outstanding feature of the present invention and marked improvement, only be the present invention is described and never limit the present invention.
Embodiment 1
With 1g LiCoO
2Powder is put into polyacrylonitrile (molecular weight the is 1500) solution (mass percent) of 2.5g20%; abundant stirring and evenly mixing; behind the heating evaporation solvent; under air atmosphere; put into baking oven and heated 3 hours down, obtain black solid, again the black solid of gained is put into high temperature furnace at 200 ℃; 750 ℃ were heated 1 hour under nitrogen protection, just obtained the LiCoO that the surface has coated carbon
2The powdery positive electrode.In active material: acetylene black: the ratio (mass percent) that adhesive equals 85:10:5 is mixed and made into cathode film, with the lithium sheet as negative pole, with Cellgard 2300 perforated membranes as barrier film, with the LiPF of 1mol/L
6/ EC+DMC (volume ratio 1:1) mixed solution is made electrolyte, is assembled into button cell.On the program control full-automatic electrochemical test of Land BS9300 (Wuhan gold promise electronics), carry out electrochemical property test.When current density was 1C, its specific discharge capacity was 210mAh/g, and circulating, its specific discharge capacity still remains on 92% after 300 times.
Embodiment 2
With 1g LiFePO
4Powder is put into polyacrylonitrile (molecular weight the is 1000) solution (mass percent) of 1.5g 50%; abundant stirring and evenly mixing; behind the heating evaporation solvent; under air atmosphere; put into baking oven and heated 2 hours down, obtain black solid, again the black solid of gained is put into high temperature furnace at 160 ℃; 550 ℃ were heated 1.5 hours under argon shield, just obtained the LiFePO that the surface has coated carbon
4The powdery positive electrode.In active material: acetylene black: the ratio (mass percent) that adhesive equals 80:10:10 is mixed and made into cathode film, with the lithium sheet as negative pole, with Cellgard 2300 perforated membranes as barrier film, with the LiPF of 1mol/L
6/ EC+DMC (volume ratio 1:1) mixed solution is made electrolyte, is assembled into button cell.On the program control full-automatic electrochemical test of Land BS9300 (Wuhan gold promise electronics), carry out electrochemical property test.When current density was 0.1C, its specific discharge capacity was 165mAh/g, and circulating, its specific discharge capacity still remains on 90% after 150 times.
Embodiment 3
With 1g LiMn
2O
4Powder is put into polyacrylonitrile (molecular weight the is 2000) solution (mass percent) of 2.0g 30%; abundant stirring and evenly mixing; behind the heating evaporation solvent; under air atmosphere; put into baking oven and heated 1.5 hours down, obtain black solid, again the black solid of gained is put into high temperature furnace at 220 ℃; 650 ℃ were heated 2 hours under nitrogen protection, just obtained the LiMn that the surface has coated carbon
2O
4The powdery positive electrode.In active material: acetylene black: the ratio (mass percent) that adhesive equals 80:10:10 is mixed and made into cathode film, with the lithium sheet as negative pole, with Cellgard 2300 perforated membranes as barrier film, with the LiPF of 1mol/L
6/ EC+DMC (volume ratio 1:1) mixed solution is made electrolyte, is assembled into button cell.On the program control full-automatic electrochemical test of Land BS9300 (Wuhan gold promise electronics), carry out electrochemical property test.When current density was 1C, its specific discharge capacity was 135mAh/g, and circulating, its specific discharge capacity still remains on 94% after 500 times.
Embodiment 4
With 1g LiV
2.95Ag
0.05O
8Powder is put into polyacrylonitrile (molecular weight the is 2000) solution (mass percent) of 3g 20%; abundant stirring and evenly mixing; behind the heating evaporation solvent; under air atmosphere; put into baking oven and heated 2 hours down, obtain black solid, again the black solid of gained is put into high temperature furnace at 200 ℃; 550 ℃ were heated 1 hour under nitrogen protection, just obtained the LiV that the surface has coated carbon
2.95Ag
0.05O
8The powdery positive electrode.In active material: acetylene black: the ratio (mass percent) that adhesive equals 80:10:10 is mixed and made into cathode film, with the lithium sheet as negative pole, with the Cellgard2300 perforated membrane as barrier film, with the LiPF of 1mol/L
6/ EC+DMC (volume ratio 1:1) mixed solution is made electrolyte, is assembled into button cell.On the program control full-automatic electrochemical test of Land BS9300 (Wuhan gold promise electronics), carry out electrochemical property test.When current density was 0.5C, its specific discharge capacity was 254mAh/g, and circulating, its specific discharge capacity still remains on 85% after 200 times.
Embodiment 5
With 1g LiMn
1/3Co
1/3Ni
1/3O
4Powder is put into polyacrylonitrile (molecular weight the is 5000) solution (mass percent) of 2.0g10%; abundant stirring and evenly mixing; behind the heating evaporation solvent; under air atmosphere; put into baking oven and heated 2 hours down, obtain black solid, again the black solid of gained is put into high temperature furnace at 200 ℃; 600 ℃ were heated 3 hours under nitrogen protection, just obtained the LiMn that the surface has coated carbon
1/3Co
1/3Ni
1/3O
4The powdery positive electrode.In active material: acetylene black: the ratio (mass percent) that adhesive equals 85:10:5 is mixed and made into cathode film, with the lithium sheet as negative pole, with Cellgard 2300 perforated membranes as barrier film, with the LiPF of 1mol/L
6/ EC+DMC (volume ratio 1:1) mixed solution is made electrolyte, is assembled into button cell.On the program control full-automatic electrochemical test of Land BS9300 (Wuhan gold promise electronics), carry out electrochemical property test.When current density was 1C, its specific discharge capacity was 145mAh/g, and circulating, its specific discharge capacity still remains on 97% after 100 times.
Claims (6)
1. the preparation method of a lithium ion battery positive material coated with carbon; it is characterized in that: the certain amount of lithium ion battery positive powder is put into polyacrylonitrile solution; abundant stirring and evenly mixing; behind the heating evaporation solvent; under air atmosphere; putting into baking oven heated 2～4 hours down at 150～300 ℃; obtain black solid; again the black solid of gained is put into high temperature furnace; 400～1200 ℃ were heated 0.5～4 hour under inert gas shielding, just obtained the lithium ion battery powdery positive electrode that the surface has coated carbon.
2. the preparation method of a kind of lithium ion battery positive material coated with carbon according to claim 1, it is characterized in that: anode material for lithium-ion batteries is LiCoO
2, LiFePO
4, LiNiO
2, LiV
3O
8, LiMn
2O
4Or their doped derivatives.
3. the preparation method of a kind of lithium ion battery positive material coated with carbon according to claim 1, it is characterized in that: the molecular weight of polyacrylonitrile is 1000～30000, the weight percent concentration of polyacrylonitrile solution is 5～100%.
4. the preparation method of a kind of lithium ion battery positive material coated with carbon according to claim 1, it is characterized in that: the weight ratio of polyacrylonitrile and lithium ion battery positive material powder is 25～95%.
5. the preparation method of a kind of lithium ion battery positive material coated with carbon according to claim 1, it is characterized in that: inert gas is nitrogen or argon gas.
6. the preparation method of a kind of lithium ion battery positive material coated with carbon according to claim 2 is characterized in that: anode material for lithium-ion batteries LiCoO
2, LiFePO
4, LiNiO
2, LiV
3O
8, LiMn
2O
4Doped derivatives, be partly to substitute the compound that is generated behind Co, Fe in the above composite oxides, Ni, V, the Mn with one or more metallic elements among Mg, Ti, Cr, Al, Cu, Ag, Zr, Nb, the W.
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|---|---|---|---|
| CN200910106325A CN101521276A (en) | 2009-03-30 | 2009-03-30 | Method for producing lithium ion battery positive material coated with carbon |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910106325A CN101521276A (en) | 2009-03-30 | 2009-03-30 | Method for producing lithium ion battery positive material coated with carbon |
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|---|---|
| CN101521276A true CN101521276A (en) | 2009-09-02 |
Family
ID=41081738
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Cited By (17)
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| CN102074692A (en) * | 2010-12-31 | 2011-05-25 | 深圳大学 | Preparation method for similar graphene doped lithium ion battery positive electrode material |
| CN102263239A (en) * | 2011-06-21 | 2011-11-30 | 刘剑洪 | Graphene-like clad and doped lithium manganate composite cathode material and preparation method |
| CN102280617A (en) * | 2011-07-06 | 2011-12-14 | 中国科学院过程工程研究所 | Carbon material modified composite lithium manganese oxide cathode material applied to lithium ion battery and preparation method thereof |
| CN102280613A (en) * | 2011-06-23 | 2011-12-14 | 浙江大学 | Preparation method of lithium ion cell anode material coating carbon fiber and product thereof |
| CN102412395A (en) * | 2010-12-24 | 2012-04-11 | 无锡力泰能源科技股份有限公司 | Modified spinel lithium manganate for secondary lithium ion battery and preparation method thereof |
| CN102479950A (en) * | 2010-11-23 | 2012-05-30 | 中国科学院物理研究所 | Titanium niobate composite material, preparation method thereof, and cathode and battery containing the same |
| CN103730652A (en) * | 2013-12-27 | 2014-04-16 | 广西科技大学 | Lithium battery, lithium battery cathode material and preparation method of lithium battery cathode material |
| CN103972493A (en) * | 2014-04-02 | 2014-08-06 | 芜湖浙鑫新能源有限公司 | Preparation method of carbon-coated doping-modification ternary composite cathode material for lithium ion battery |
| CN104681782A (en) * | 2015-01-29 | 2015-06-03 | 北大先行科技产业有限公司 | Lithium ion secondary battery composite positive material and preparation method thereof |
| CN104701531A (en) * | 2015-02-04 | 2015-06-10 | 武汉理工大学 | In-situ carbon-coating hexagon K0.7[Fe0.5Mn0.5]O2 nano material as well as preparation method and application thereof |
| CN107464924A (en) * | 2017-07-24 | 2017-12-12 | 江苏大学 | A kind of sheet oxygen defect lithium vanadate anode material and preparation method thereof |
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| CN110190273A (en) * | 2019-07-10 | 2019-08-30 | 深圳市本征方程石墨烯技术股份有限公司 | A kind of manganate cathode material for lithium and preparation method thereof of graphene doping |
| CN110311128A (en) * | 2019-07-10 | 2019-10-08 | 深圳市本征方程石墨烯技术股份有限公司 | A kind of lithium cobaltate cathode material and preparation method thereof of graphene doping |
| CN113363488A (en) * | 2021-06-02 | 2021-09-07 | 北京理工大学 | Method for preparing homopolymer low-temperature carbon-coated electrode material based on 2-acrylonitrile |
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2009
- 2009-03-30 CN CN200910106325A patent/CN101521276A/en active Pending
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| CN102479950A (en) * | 2010-11-23 | 2012-05-30 | 中国科学院物理研究所 | Titanium niobate composite material, preparation method thereof, and cathode and battery containing the same |
| CN102412395A (en) * | 2010-12-24 | 2012-04-11 | 无锡力泰能源科技股份有限公司 | Modified spinel lithium manganate for secondary lithium ion battery and preparation method thereof |
| WO2012089085A1 (en) * | 2010-12-31 | 2012-07-05 | 深圳大学 | Method for preparing graphene-like doped positive electrode material of lithium-ion battery |
| CN102074692A (en) * | 2010-12-31 | 2011-05-25 | 深圳大学 | Preparation method for similar graphene doped lithium ion battery positive electrode material |
| CN102074692B (en) * | 2010-12-31 | 2013-10-30 | 深圳大学 | Preparation method for similar graphene doped lithium ion battery positive electrode material |
| US20140103264A1 (en) * | 2011-06-21 | 2014-04-17 | Jianhong Liu | Positive electrode materials for lithium-ion batteries and method for preparing the same |
| CN102263239A (en) * | 2011-06-21 | 2011-11-30 | 刘剑洪 | Graphene-like clad and doped lithium manganate composite cathode material and preparation method |
| US9379382B2 (en) * | 2011-06-21 | 2016-06-28 | Shenzhen Eigen-Equation Graphene Technology Co., Ltd. | Positive electrode materials for lithium-ion batteries and method for preparing the same |
| CN102263239B (en) * | 2011-06-21 | 2016-02-10 | 深圳市本征方程石墨烯技术股份有限公司 | One kind graphene coated adulterated lithium manganate composite positive pole and preparation method thereof |
| CN102280613A (en) * | 2011-06-23 | 2011-12-14 | 浙江大学 | Preparation method of lithium ion cell anode material coating carbon fiber and product thereof |
| CN102280613B (en) * | 2011-06-23 | 2013-10-02 | 浙江大学 | Preparation method of lithium ion cell anode material coating carbon fiber and product thereof |
| CN102280617A (en) * | 2011-07-06 | 2011-12-14 | 中国科学院过程工程研究所 | Carbon material modified composite lithium manganese oxide cathode material applied to lithium ion battery and preparation method thereof |
| CN103730652A (en) * | 2013-12-27 | 2014-04-16 | 广西科技大学 | Lithium battery, lithium battery cathode material and preparation method of lithium battery cathode material |
| CN103972493A (en) * | 2014-04-02 | 2014-08-06 | 芜湖浙鑫新能源有限公司 | Preparation method of carbon-coated doping-modification ternary composite cathode material for lithium ion battery |
| CN104681782A (en) * | 2015-01-29 | 2015-06-03 | 北大先行科技产业有限公司 | Lithium ion secondary battery composite positive material and preparation method thereof |
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| CN113363488A (en) * | 2021-06-02 | 2021-09-07 | 北京理工大学 | Method for preparing homopolymer low-temperature carbon-coated electrode material based on 2-acrylonitrile |
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